Preparation method of modified PBT-DTY elastic fiber with enhanced elasticity

Abstract

The present application relates to the technical field of PBT-DTY elastic fiber preparation, in particular to a preparation method of an elastic enhancement type modified PBT-DTY elastic fiber, which comprises the following steps: S1, dosing; S2, preparing a composite fiber: S2-1, preparing a fiber matrix, S2-2, preparing a composite yarn, S2-3, spinning compounding, S3, stretching and setting, and S4, post-treatment; by adjusting the content of the elastomer modifier, the reinforcing agent and the stabilizer, the performance of the fiber can be changed to adapt to different application requirements; by adding the reinforcing agent, the durability of the fiber can be significantly improved; by spinning compounding the fiber matrix and the composite yarn, the elasticity of the PBT-DTY elastic fiber can be effectively improved; the PBT-DTY elastic fiber prepared by the method can strengthen the elastic performance of the fiber, ensure the stability and durability of the fiber, and is suitable for large-scale production.

Description

Technical Field

[0001] This invention relates to the field of PBT-DTY elastic fiber preparation technology, specifically to a method for preparing elastic-enhanced modified PBT-DTY elastic fiber. Background Technology

[0002] There are two process technologies for the production of PBT polyester: direct esterification of PTA and transesterification of DMT. Compared with the DMT transesterification method, direct esterification of PTA is more environmentally friendly, has a shorter preparation cycle, lower construction costs, and higher economic added value.

[0003] The PBT three-reactor process refers to a continuous reaction process using three reactors in the production of polybutylene terephthalate (PBT). The specific steps of the PBT three-reactor process are as follows: The first reactor (ester exchange reactor) performs the ester exchange reaction: terephthalic acid (PTA) and butanediol are added to the ester exchange reactor along with a catalyst, commonly a zinc or tin compound. Under specific temperature and pressure conditions, the ester exchange reaction takes place. In this reaction, PTA and butanediol undergo ester exchange to produce the intermediate product, polybutylene terephthalate.

[0004] The process transitions to a second reactor (polymerization reactor) for polymerization: the intermediate product from the transesterification reactor is transferred to the polymerization reactor. A polymerization catalyst is added, typically a metal salt catalyst such as titanium or zinc. The polymerization reaction takes place under specific temperature and pressure conditions. The intermediate product in the polymerization reactor undergoes polymerization to produce PBT polymer. The process then transitions to a third reactor (post-processing reactor) for post-processing: the polymer from the polymerization reactor is transferred to the post-processing reactor. Post-processing operations are performed, such as polymer decomposition and purification at high temperatures, to remove impurities and adjust product properties. The reaction conditions and catalyst selection parameters in the PBT three-reactor process are adjusted and optimized according to the specific process and equipment to ensure the production of PBT products that meet requirements. This process enables continuous and efficient production, improving product quality and production efficiency, and is widely used in the production of PBT resin. However, the elasticity properties of existing PBT-DTY elastic fiber fabrics still need to be improved and strengthened. Summary of the Invention

[0005] This invention addresses the shortcomings of existing technologies by providing a method for preparing elastic-enhanced modified PBT-DTY elastic fibers, comprising the following steps:

[0006] S1, Ingredients

[0007] Prepare 10-15% elastomer modifier, 5-10% reinforcing agent, 0.1-1% stabilizer, and the balance PBT by weight percentage; the elastomer modifier is polybutylene succinate elastomer; the reinforcing agent is glass fiber or carbon fiber; the stabilizer is antioxidant or UV stabilizer.

[0008] S2, Preparation of composite fibers

[0009] S2-1, Preparation of fiber matrix

[0010] The PBT, reinforcing agent, stabilizer and elastomer modifier are mixed in the proportions described in step S1 and then placed in a high-shear mixer to obtain a mixture; the mixture is fed into an extruder and extruded into continuous fibers at a temperature of 200-240°C to obtain a fiber matrix.

[0011] S2-2, Preparation of composite yarn: Polymerize styrene and glycidyl methacrylate in a mass ratio of 1 to 4:1 to obtain polystyrene; spin polystyrene and polyurethane into composite yarn in a mass ratio of 1:4 to 9, and then soak it in an inorganic alkali mixed solution for 5 to 15 hours to obtain composite yarn;

[0012] S2-3, Spinning and compounding: The composite yarn and the fiber matrix are spun and compounded at a mass ratio of 1:6 to 9 to obtain composite fiber;

[0013] S3, Stretching and Shaping

[0014] The composite fibers described in steps S2-3 are stretched and shaped using a texturing false twisting machine. The tension of the composite fibers is adjusted and controlled by an auxiliary roller to obtain an elastic material.

[0015] S4, Post-processing

[0016] The elastic material described in step S3 is cut and impurity removed to obtain the desired fiber morphology and length, thus obtaining modified elastic fiber.

[0017] Description: By adding elastomer modifiers and undergoing stretching and shaping treatment, the prepared modified elastic fibers possess excellent elasticity and flexibility, allowing them to better adapt to stress and shape changes during use, providing better comfort and plasticity. Introducing reinforcing agents, such as glass fibers or carbon fibers, can significantly improve the strength and stiffness of the fibers, increasing their load-bearing capacity and durability. The use of stabilizers can improve the fiber's stability against external environmental factors such as oxidation and ultraviolet radiation, extending its service life and reducing aging and damage during use. By combining different materials and processing steps, the modified elastic fibers exhibit excellent elasticity, reinforcement, stability, and adjustability, meeting the requirements of various application fields for elastic fibers.

[0018] Further, the stretching and shaping method described in step S3 is as follows: the composite fiber is stretched using a texturing false twisting machine, and POY oil is coated on the surface of the composite fiber, with the coating amount controlled to be 0.2-0.4% of the composite fiber mass; the stretching temperature is adjusted from room temperature to 250-350℃, DR is 1.2-1.6m / min, D / Y ratio is 1.5-2, stretching speed is 5-20s / time, and stretching time is 10-30min to obtain elastic fiber material; the elastic fiber material is sent into a hot box, the temperature is adjusted to 150-250℃, and it is kept at this temperature for 3-7h before cooling and shaping.

[0019] Explanation: Stretching through a texturing and false twisting machine makes the fibers more compact and stretched, thereby improving their strength and elasticity. During stretching, coating the fiber surface with POY oil effectively reduces friction between fibers, improving their feel and appearance, and enhancing their quality and performance. DR refers to the stretching ratio between the W1 roller (front roller of the texturing and false twisting machine) and the W2 roller (rear roller of the texturing and false twisting machine). The D / Y ratio is the ratio of the surface velocity of the friction disc in the false twister to the velocity of the filament leaving the false twister. By controlling parameters such as stretching temperature, DR, D / Y ratio, stretching speed, and stretching time, the size and shape of the fibers can be precisely controlled to meet the manufacturing requirements of different fiber products. Insulating the elastic fiber material in a hot box further strengthens the bond between fiber molecules, enhancing the fiber's stability and durability.

[0020] Furthermore, the spinning composite method is one of wet spinning, dry spinning, or melt spinning.

[0021] Note: Different spinning composite methods can control the quality and performance of fibers according to requirements. Wet spinning allows for the control of fiber quality through parameters such as solution concentration and pH value during the spinning process; dry spinning provides more direct control over fiber shape and size; melt spinning allows for the control of fiber melting point and elongation.

[0022] Further, the preparation method of polystyrene in step S2-2 is as follows: styrene and glycidyl methacrylate are mixed in the specified proportion and soaked in a dispersant solution of 0.1-0.3% wt, and then an initiator of 1-10% by mass of the dispersant solution is added to carry out a polymerization reaction to obtain polystyrene.

[0023] Note: By mixing styrene and glycidyl methacrylate and soaking them in a dispersant solution, the dispersibility of the polymer during polymerization can be optimized. The proportioning and processing methods used in the preparation method can control the performance and quality of polystyrene to meet specific application requirements.

[0024] Furthermore, the dispersant is one of PVA, gelatin, alginate, or carboxymethyl cellulose; the initiator is AIBN.

[0025] Note: PVA, gelatin, alginate, and carboxymethyl cellulose can all serve as excellent dispersants, effectively dispersing styrene and glycidyl methacrylate in solution, ensuring uniform mixing and stability during polymerization. They can also create appropriate viscosity and flowability in solution. This facilitates mixing and dispersion of raw materials and maintains the homogeneity of the polymerization reaction. Natural substances such as PVA, gelatin, alginate, and carboxymethyl cellulose have good biodegradability and environmental friendliness, with minimal negative impact on the environment. AIBN is a commonly used free radical initiator that generates free radicals to initiate polymerization, effectively promoting the formation of polystyrene.

[0026] Furthermore, the polymerization reaction is carried out by holding the reaction at a temperature of 80-90°C for 2-4 hours, followed by holding the reaction at a temperature of 85-95°C for 3-6 hours.

[0027] Note: Appropriate holding time can ensure that the polymerization reaction proceeds fully, thereby obtaining higher yields and desired product properties, promoting the polymerization reaction, improving reaction efficiency, and reducing the possibility of side reactions and product degradation.

[0028] Further, the method for preparing the inorganic alkali mixed solution in step S2-2 is as follows: 4-6% of the inorganic alkali by mass of the composite fiber is uniformly mixed with an antibacterial agent with a concentration of 25-35 g / L, wherein the mass ratio of the inorganic alkali to the antibacterial agent is 1:10-15; the inorganic alkali is one of sodium bicarbonate, sodium carbonate, or sodium hydroxide.

[0029] Note: Adding antibacterial agents can effectively inhibit the growth of bacteria, fungi and other microorganisms, thereby enhancing the antibacterial properties of fibers and products and improving the hygiene and safety of products; the inorganic alkali has appropriate solubility and can be fully mixed with other components in solution to promote the grafting reaction.

[0030] Furthermore, the antibacterial agent is one or more combinations of polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, polymeric guanidine hydrochloride, hydrochloride, phosphate, and gluconate.

[0031] Note: Antimicrobial agents include various types such as polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, polymeric guanidine hydrochloride, hydrochloride, phosphate, and gluconate. These antimicrobial agents typically have broad-spectrum antimicrobial activity, effectively inhibiting the growth of various bacteria, fungi, and other microorganisms. Combining multiple antimicrobial agents can produce a synergistic effect, further enhancing antimicrobial performance and thus better protecting fibers and products from microbial contamination. They also exhibit good durability and stability, forming a layer with sustained antimicrobial capabilities on the surface of elastic fibers, providing long-term antimicrobial protection.

[0032] Compared with the prior art, the beneficial effects of the present invention are:

[0033] This invention modifies fiber properties by adjusting the content of elastomer modifiers, reinforcing agents, and stabilizers to adapt to different application requirements. Adding reinforcing agents significantly improves fiber durability, enhancing its load-bearing capacity and service life. Adding composite yarns to the fiber matrix for spinning effectively improves the elasticity of PBT-DTY elastic fibers. Adding stabilizers to the fiber material improves its stability against environmental factors such as oxidation and ultraviolet radiation, extending fiber life and reducing aging and breakage during use. This method utilizes traditional textile processes and equipment, making it easy to implement and control. This invention allows for appropriate mixing, extrusion, spinning, and stretching / setting treatments based on desired fiber properties and performance, ensuring a stable and controllable fiber preparation process. PBT-DTY elastic fibers prepared using this method exhibit enhanced elasticity, guaranteeing fiber stability and durability, making them suitable for large-scale production. Detailed Implementation

[0034] The present invention will now be described in more detail with reference to specific embodiments, so as to better demonstrate the advantages of the present invention.

[0035] Example 1

[0036] A method for preparing elastic-enhanced modified PBT-DTY elastic fiber includes the following steps:

[0037] S1, Ingredients

[0038] Prepare 12.5% ​​elastomer modifier, 7.5% reinforcing agent, 0.5% stabilizer, and the balance PBT by weight percentage; the elastomer modifier is polybutylene succinate elastomer; the reinforcing agent is carbon fiber; and the stabilizer is an ultraviolet stabilizer.

[0039] S2, Preparation of composite fibers

[0040] S2-1, Preparation of fiber matrix

[0041] The PBT, reinforcing agent, stabilizer, and elastomer modifier are mixed in the proportions described in step S1 and then placed in a high-shear mixer to obtain a mixture. The mixture is then fed into an extruder and extruded into continuous fibers at a temperature of 220°C to obtain a fiber matrix.

[0042] S2-2, Preparation of composite yarn: Styrene and glycidyl methacrylate are polymerized at a mass ratio of 2.5:1 to obtain polystyrene; polystyrene is then spun into composite yarn with polyurethane at a mass ratio of 1:6.5, and subsequently immersed in an inorganic alkali mixed solution for 10 hours to obtain composite yarn; the spinning composite method is wet spinning.

[0043] The preparation method of the polystyrene is as follows: styrene and glycidyl methacrylate are mixed in the specified proportion and soaked in a 0.2% wt dispersant solution. Then, an initiator accounting for 5.5% of the mass of the dispersant solution is added to carry out a polymerization reaction. The reaction is kept at 85°C for 3 hours and then kept at 90°C for 4.5 hours to obtain polystyrene.

[0044] The dispersant is PVA; the initiator is AIBN;

[0045] The inorganic alkali mixed solution is prepared by uniformly mixing an inorganic alkali accounting for 5% of the mass of the composite fiber with an antibacterial agent at a concentration of 30 g / L, wherein the mass ratio of the inorganic alkali to the antibacterial agent is 1:12.5; the inorganic alkali is sodium bicarbonate; and the antibacterial agent is polyhexamethylene biguanide hydrochloride.

[0046] S2-3, Spinning and compounding: The composite yarn and the fiber matrix are dry spun and compounded at a mass ratio of 1:7.5 to obtain composite fiber;

[0047] S3, Stretching and Shaping

[0048] The composite fibers described in steps S2-3 are stretched and shaped using a texturing false twisting machine. The tension of the composite fibers is adjusted and controlled by an auxiliary roller to obtain an elastic material.

[0049] The stretching and shaping method is as follows: the composite fiber is stretched using a texturing and false-twisting machine; POY oil is coated on the surface of the composite fiber, and the amount of coating is controlled to be 0.3% of the composite fiber mass; the stretching temperature is adjusted from room temperature to 300℃, DR is 1.4m / min, D / Y ratio is 1.75, stretching speed is 15s / cycle, and stretching time is 20min to obtain elastic fiber material; the elastic fiber material is sent into a hot box, the temperature is adjusted to 200℃, and it is kept at this temperature for 5 hours before cooling and shaping.

[0050] S4, Post-processing

[0051] The elastic material described in step S3 is cut and impurity removed to obtain the desired fiber morphology and length, thus obtaining modified elastic fiber.

[0052] Example 2

[0053] The difference between this embodiment and Embodiment 1 is that 10% elastomer modifier, 5% reinforcing agent, 0.1% stabilizer, and the balance PBT are prepared.

[0054] Example 3

[0055] The difference between this embodiment and Embodiment 1 is that 15% elastomer modifier, 10% reinforcing agent, 1% stabilizer, and the balance PBT are prepared.

[0056] Example 4

[0057] The difference between this embodiment and Example 1 is that the mass ratio of styrene and glycidyl methacrylate is 1:1 to obtain polystyrene; the polystyrene is then combined with polyurethane by spinning at a mass ratio of 1:4, and subsequently soaked in an inorganic alkali mixed solution for 5 hours to obtain composite yarn.

[0058] Example 5

[0059] The difference between this embodiment and Example 1 is that the mass ratio of styrene to glycidyl methacrylate is 4:1 to obtain polystyrene; the polystyrene is then combined with polyurethane by spinning at a mass ratio of 1:9, and subsequently soaked in an inorganic alkali mixed solution for 15 hours to obtain composite yarn.

[0060] Example 6

[0061] The difference between this embodiment and Example 1 is that styrene and glycidyl methacrylate are mixed in the specified ratio and soaked in a 0.1% wt dispersant solution. Then, an initiator accounting for 1% of the mass of the dispersant solution is added to carry out a polymerization reaction. The reaction is kept at 80°C for 2 hours and then kept at 85°C for 3 hours to obtain polystyrene.

[0062] Example 7

[0063] The difference between this embodiment and Example 1 is that styrene and glycidyl methacrylate are mixed in the specified ratio and soaked in a 0.3% wt dispersant solution. Then, an initiator accounting for 10% of the mass of the dispersant solution is added to carry out a polymerization reaction. The reaction is kept at 90°C for 4 hours and then kept at 95°C for 6 hours to obtain polystyrene.

[0064] Example 8

[0065] The difference between this embodiment and Embodiment 1 is that POY oil is coated on the surface of the composite fiber, and the amount of coating is controlled to be 0.2% of the mass of the composite fiber; the stretching temperature is adjusted from room temperature to 250°C, DR is 1.2 m / min, D / Y ratio is 1.5, stretching speed is 5 s / time, and stretching time is 10 min to obtain elastic fiber material; the elastic fiber material is sent into a hot box, the temperature is adjusted to 150°C, and after holding for 3 hours, it is cooled and shaped.

[0066] Example 9

[0067] The difference between this embodiment and Embodiment 1 is that POY oil is coated on the surface of the composite fiber, and the amount of coating is controlled to be 0.4% of the mass of the composite fiber; the stretching temperature is adjusted from room temperature to 350°C, DR is 1.6m / min, D / Y ratio is 2, stretching speed is 20s / time, and stretching time is 30min to obtain elastic fiber material; the elastic fiber material is sent into a hot box, the temperature is adjusted to 250°C, and after holding at the temperature for 7h, it is cooled and shaped.

[0068] Experimental example:

[0069] The elastic fiber samples obtained in Examples 1-5, 8, 9 and the comparative example were tested, and the results of the specific performance tests are detailed in Table 1.

[0070] The comparative example differs from Example 1 in that no composite yarn was prepared and the fiber matrix was not spun into composite yarn.

[0071] Table 1: Performance Test Table for 8 Different Elastic Fibers

[0072]

[0073] 1. To investigate the effect of the ratio parameters of the fiber matrix on the properties of the prepared elastic fiber.

[0074] Conclusion: As can be seen from the data in Table 1, the elastic fiber prepared by using the fiber matrix ratio in Example 1 has a better elongation at break. Compared with Example 3, Example 2 has a better breaking strength. Overall, the elastic fiber in Example 1 has better comprehensive performance.

[0075] 2. To investigate the effect of the ratio parameters of the composite yarn preparation on the properties of the prepared elastic fiber.

[0076] Conclusion: As can be seen from the data in Table 1, compared with Example 5, the elastic fiber prepared by using the composite yarn ratio in Example 4 has a better breaking elongation. Overall, the elastic fiber in Example 1 has better comprehensive performance.

[0077] 3. Investigate the effects of process parameters for stretching and texturing composite fibers on the properties of the prepared elastic fibers.

[0078] As can be seen from the data in Table 1, compared with Example 1, Example 1 has better overall performance. Compared with Examples 1 and 9, Example 8 has the highest elongation at break and Example 9 has the lowest elongation at break and the highest curl shrinkage. It can be seen that the higher the stretch ratio, the lower the elongation at break, and the curl shrinkage is slightly increased.

Claims

1. A method for preparing elastic-enhanced modified PBT-DTY elastic fiber, characterized in that, Includes the following steps: S1, Ingredients Prepare 10-15% elastomer modifier, 5-10% reinforcing agent, 0.1-1% stabilizer, and the balance PBT by weight percentage; the elastomer modifier is polybutylene succinate elastomer; the reinforcing agent is glass fiber or carbon fiber; the stabilizer is antioxidant or UV stabilizer. S2, Preparation of composite fibers S2-1. Preparation of fiber matrix: The PBT, reinforcing agent, stabilizer and elastomer modifier are mixed in the proportions in step S1 and then placed in a high-shear mixer to obtain a mixture; the mixture is fed into an extruder and extruded into continuous fibers at a temperature of 200~240℃ to obtain a fiber matrix. S2-2, Preparation of composite yarn: Styrene and glycidyl methacrylate are polymerized at a mass ratio of 1-4:1, and the mixture is immersed in a 0.1-0.3% wt dispersant solution. Then, an initiator at a mass of 1-10% of the dispersant solution is added to carry out the polymerization reaction, yielding polystyrene. Polystyrene is then spun into composite yarn with polyurethane at a mass ratio of 1:4-9. The composite yarn is then immersed in an inorganic alkali mixture for 5-15 hours to obtain the composite yarn. The inorganic alkali mixture is prepared by uniformly mixing 4-6% of the inorganic alkali (by mass of the composite fiber) with an antibacterial agent at a concentration of 25-35 g / L, at a mass ratio of 1:10-15. The inorganic alkali is one of sodium bicarbonate, sodium carbonate, or sodium hydroxide. S2-3, Spinning and compounding: The composite yarn and the fiber matrix are spun and compounded at a mass ratio of 1:6~9 to obtain composite fiber; S3, Stretching and Shaping The composite fibers described in steps S2-3 are stretched and shaped using a texturing and false-twisting machine. The tension of the composite fibers is adjusted and controlled using auxiliary rollers to obtain an elastic material. The stretching and shaping method is as follows: the composite fibers are stretched using a texturing and false-twisting machine, and POY oil is coated on the surface of the composite fibers, with the coating amount controlled to be 0.2~0.4% of the composite fiber mass. The stretching temperature is adjusted from room temperature to 250~350℃, the DR is 1.2~1.6m / min, the D / Y ratio is 1.5~2, the stretching speed is 5~20s / time, and the stretching time is 10~30min to obtain the elastic fiber material. The elastic fiber material is fed into a hot box, the temperature is adjusted to 150~250℃, and it is kept at the temperature for 3~7 hours before cooling and shaping. S4, Post-processing The elastic material described in step S3 is cut and impurity removed to obtain the desired fiber morphology and length, thus obtaining modified elastic fiber.

2. The method for preparing an elastic-enhanced modified PBT-DTY elastic fiber according to claim 1, characterized in that, The spinning composite method is one of wet spinning, dry spinning, or melt spinning.

3. The method for preparing an elastic-enhanced modified PBT-DTY elastic fiber according to claim 1, characterized in that, The dispersant is one of PVA, gelatin, alginate, or carboxymethyl cellulose; the initiator is AIBN.

4. The method for preparing an elastic-enhanced modified PBT-DTY elastic fiber according to claim 1, characterized in that, The polymerization reaction is carried out by holding the reaction at 80-90°C for 2-4 hours, followed by holding the reaction at 85-95°C for 3-6 hours.

5. The method for preparing an elastic-enhanced modified PBT-DTY elastic fiber according to claim 1, characterized in that, The antibacterial agent is one or a combination of polyhexamethylene biguanide hydrochloride, polyhexamethylene guanidine hydrochloride, polymeric guanidine hydrochloride, hydrochloride, phosphate, and gluconate.

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